HPLC-MS/MS同时测定芪龙胶囊中6个有效成分的含量

Simultaneous determination of six active ingredients in Qilong capsules by HPLC-MS/MS

目的:建立高效液相色谱-串联杆质谱法(HPLC-MS/MS)同时测定芪龙胶囊中丹参酚酸B、芍药苷、丹参酮ⅡA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷6个有效成分的含量。方法:采用CAPCELL PAK C18色谱柱(2.0 mm×150 mm,5μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,流速0.4 mL·min^-1,柱温30℃,进样量10μL;质谱采用电喷雾电离源(ESI^+),多反应监测模式(MRM),离子源电压5 kV,离子源温度450℃,气帘气103.4 kPa,雾化气344.7 kPa,辅助气379.2 kPa。结果:所测6个有效成分在测定质量浓度范围内线性关系良好(r>0.9929);平均加样回收率为91.2%~104.8%,RSD为1.3%~5.1%。13批芪龙胶囊中丹参酚酸B、芍药苷、丹参酮ⅡA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷的含量范围分别为0.164~0.323、0.561~0.952、0.009~0.030、0.113~0.397、0.014~0.284、0.041~0.138 mg·粒^-1。结论:该方法适用于芪龙胶囊成药中丹参酚酸B、芍药苷、丹参酮ⅡA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷6个有效成分含量的同时测定,可用于芪龙胶囊的质量控制。

Objective:To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for simultaneous determination of salvianolic acid B,paeoniflorin,tanshinoneⅡA,astragaloside A,amygdalin and calycosin-7-glucoside in Qilong capsules.Methods:The contents of six active ingredients in Qilong capsules were determined by CAPCELL PAK C18 column(2.0 mm×150 mm,5μm)with 0.1%formic acid solution-acetonitrile as mobile phase using gradient elution at a flow rate of 0.4 mL·min^-1.The column temperature was 30℃and the injection volume was 10μL.ESI+scan combined with multi-reaction monitoring mode(MRM)was adopted and the instrument parameters were as follows:ionsource voltage:5 kV;temperature:450℃;curtain gas:103.4 kPa;atomized gas:344.7 kPa;auxiliary gas:379.2 kPa.Results:The linear relationship of the six active ingredients was good(r>0.9929).The average recoveries were 91.2%-104.8%with RSD of 1.3%-5.1%.The contents of salvianolic acid B,paeoniflorin,tanshinoneⅡA,astragaloside A,amygdalin and calycosin-7-glucoside in 13 batches of Qilong capsules were 0.164-0.323,0.561-0.952,0.009-0.030,0.113-0.397,0.014-0.284 and 0.041-0.138 mg per capsule,respectively.Conclusion:The method is suitable for the simultaneous determination of salvianolic acid B,paeoniflorin,tanshinoneⅡA,astragaloside A,amygdalin and calycosin-7-glucoside in Qilong capsules.It can be used for the quality control of Qilong capsules.